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Preparation method of benzyl acetate

A technology of benzyl acetate and sodium acetate, applied in the field of benzyl acetate preparation, can solve problems such as affecting the aroma of benzyl acetate, side reactions, etc., and achieve the effects of improving reaction yield and conversion rate, pure aroma and good purity

Inactive Publication Date: 2015-03-11
FUZHOU FUDA HUIXIANG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the synthesis of benzyl acetate from benzyl chloride, the hydrolysis of benzyl chloride is often accompanied by side reactions, and its by-products, such as benzaldehyde and benzyl alcohol, will affect the aroma of benzyl acetate

Method used

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  • Preparation method of benzyl acetate

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preparation example Construction

[0030] see figure 1 , is a flowchart of the preparation method of benzyl acetate described in one embodiment of the present invention. The method comprises the steps of:

[0031] S1, the organic amine reacts with excess benzyl chloride to obtain a phase transfer catalyst raw material solution;

[0032] The reaction conditions are: react at 60-90°C for 15-60 minutes, and the molar ratio of benzyl chloride to organic amine is 1:0.01-0.04. And, the organic amine is dimethylamine, trimethylamine, ethylamine.

[0033] S2. Adding sodium acetate, water, and sodium carbonate to the phase transfer catalyst raw material solution for esterification to obtain the first crude product of benzyl acetate;

[0034] The mol ratio of sodium acetate, water, sodium carbonate in the described esterification reaction is 1.05-1.25:0.4-0.5:0.01-0.03; The mass ratio of each reactant added in the described benzyl chloride and esterification reaction is 1: 1.05-1.25:0.4-0.5:0.01-0.03. The temperatur...

no. 1 example

[0050] Weigh 300g of benzyl chloride and 6g of ethylamine into the reactor, keep the temperature at 85°C, stir and react for 20 minutes, put 235g of anhydrous sodium acetate, 17g of water, and 4g of sodium carbonate into the reactor, raise the temperature to 120°C, and stir for 2.5 Hour. The first crude product of benzyl acetate was obtained after the reaction was completed, and the second crude product of benzyl acetate was obtained by washing with water.

[0051]In the second crude product of benzyl acetate of 346g, add 103.8g mass fraction and be 5% sodium carbonate aqueous solution, react at 120 ℃ for 1 hour, separate layers to obtain the organic phase; then add 173g saturated aqueous sodium bisulfite solution in the organic phase The reaction was stirred at room temperature for 1 hour, and the layers were separated to obtain the upper organic layer. Stir and react the organic layer with 14g acetic acid and 4g cationic resin at 80°C for 1.5 hours, filter, the obtained fil...

no. 2 example

[0054] Weigh 400g of benzyl chloride and 8g of dimethylamine into the reaction kettle, keep the temperature at 75°C, stir and react for 30 minutes, put 300g of anhydrous sodium acetate, 20g of water, and 4g of sodium carbonate into the reaction kettle, raise the temperature to 110°C, and stir for reaction 3 hours. The first crude product of benzyl acetate was obtained after the reaction was completed, and the second crude product of benzyl acetate was obtained by washing with water.

[0055] In the second crude product of benzyl acetate of 453, adding 182.8g mass fraction is 5% aqueous sodium carbonate solution, reacted for 1 hour at 120°C, and layered to obtain the upper organic phase; then add 453g saturated aqueous sodium metabisulfite solution in the organic phase The reaction was stirred at room temperature for 1 hour, and the layers were separated to obtain the upper organic layer. Stir and react the organic layer with 28g of acetic acid and 10g of cation exchange resin...

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Abstract

The invention discloses a preparation method of benzyl acetate. The method comprises the following steps: enabling organic amine to react with excessive benzyl chloride at the temperature of 60-90 DEG C for 15-60 min so as to obtain a phase transfer catalyst feed solution; adding sodium acetate, water and sodium carbonate into the phase transfer catalyst feed solution for performing esterification reaction so as to obtain a first crude product of the benzyl acetate; washing the first crude product of the benzyl acetate with water so as to obtain a second crude product of the benzyl acetate; performing impurity removal treatment on the second crude product of the benzyl acetate so as to obtain a third crude product of the benzyl acetate; performing secondary rectification and refining operation on the third crude product of the benzyl acetate so as to obtain the pure product of the benzyl acetate. According to the invention, a homemade phase transfer catalyst is used for reaction, so that the cost is reduced, the complexity of a process route is greatly reduced, the by-product, that is benzyl alcohol, is translated into the benzyl acetate product, and the reaction yield and the conversion rate are effectively increased. The characteristics of high yield, good purity, and pure fragrance of the product are achieved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of benzyl acetate. Background technique [0002] Benzyl acetate, also known as benzyl acetate, is a colorless oily liquid that is volatile. Benzyl Acetate is an ester fragrance with a strong jasmine and fruit aroma and a sweet smell. In the fragrance industry, it is often used to prepare food flavors such as apple, raw pear, banana, jasmine, cherry, pineapple, papaya, cream, etc. It can be used in medicine, food and cosmetics as an aromatic flavoring agent or fragrance. [0003] There are generally three ways to prepare benzyl acetate in industry: the first is obtained by heating and esterifying benzyl chloride and sodium acetate under the catalysis of a catalyst, and then purified by distillation; the second is obtained by benzyl alcohol It is esterified with acetic acid and purified by distillation; the third is obtained by the action of benzaldehyde, ace...

Claims

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Application Information

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IPC IPC(8): C07C69/157C07C67/11C07C67/08
CPCC07C67/11C07C67/52C07C67/54C07C67/58C07C69/157
Inventor 钟晓琳翁汉宗周云雷郑辉东
Owner FUZHOU FUDA HUIXIANG CHEM TECH
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